Reaktion #53247

ord-71bd1248fad64cd58c8f6ed57ff96111

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigea solution obtained
  2. 2
    workup.ADDITIONwas added to the above solution
  3. 3
    ExtraktionThe aqueous solution was extracted twice with 100 ml of chloroform
  4. 4
    Waschenthe organic phase was washed with water
  5. 5
    Einengenconcentrated
  6. 6
    Sonstigean oily product was obtained
  7. 7
    EinengenThe above-obtained product was concentrated again with ethyl acetate
  8. 8
    Sonstigea solid product was obtained
  9. 9
    FiltrationThe solid product was filtered and re-slurried with diisopropyl ether

Vorschrift

Potassium perfluorobutanesulfonate (10 g) was dissolved in a mixed solvent comprising 500 ml of water and 100 ml of methanol, and a solution obtained by dissolving 7.7 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide in 50 ml of methanol was added to the above solution. The aqueous solution was extracted twice with 100 ml of chloroform, the organic phase was washed with water and concentrated, thereby an oily product was obtained. The above-obtained product was concentrated again with ethyl acetate, thereby a solid product was obtained. The solid product was filtered and re-slurried with diisopropyl ether, to thereby obtain 9 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium perfluorobutanesulfonate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858370B2uspto-grants-2005_02